CN209352933U - A kind of continuous crystalizer producing glucose and glucose production device - Google Patents

Abstract

The utility model relates to a kind of continuous crystalizer for producing glucose and glucose production devices, belong to glucose production technical field.It include: to have multiple crystallizers, crystallizer is connected between each other；It is equipped with syrup intlet at the top of crystallizer, is equipped with syrup outlet in the bottom of crystallizer；It is equipped with heat exchanger in the inside of crystallizer, the shell side of heat exchanger is connected to chilled water import and chilled water outlet respectively；Chilled water import and chilled water outlet are located at the lower part and top of heat exchanger；The syrup outlet of upper level crystallizer is connected to the syrup outlet of next stage crystallizer, and the chilled water outlet of next stage crystallizer is connected to the chilled water import of upper level crystallizer.The utility model is fed to discharging certainly and is moved under hypersaturated state using more crystallizer series connection, liquid glucose and cooling medium reverse movement, liquid glucose, and because cooling capacity is adequately utilized, energy-saving effect is more significant, and primary crystallization rate is also increased to 65% by conventional 55%.

Description

A kind of continuous crystalizer producing glucose and glucose production device

Technical field

The utility model relates to a kind of continuous crystalizer for producing glucose and glucose production devices, belong to glucose Production technical field.

Background technique

In the project of corn deep processing, the technique for producing crystal glucose mainly takes two kinds of crystallization sides for the country at present Formula: one is boilings to crystallize (concentration)；One is crystallisation by cooling.Wherein boiling, which crystallizes, need to consume steam energy, and crystallisation by cooling It is more energy-saving and environmentally friendly.But both of which is intermittently operated or the low-yield continuous operation of single machine, and there are no full device series connection to connect The method of continuous crystallization.It is badly in need of a kind of novel crystallization processes at present, can has the characteristics of ultra-large type, serialization, and can be bright The aobvious product quality and one way crystalline rate, cooling capacity of improving can be all utilized, the full intelligent automation of whole process.

Utility model content

The purpose of this utility model is: proposing a kind of new process of reverse continuous movement crystallization production glucose, uses More crystallizer series connection, liquid glucose and cooling medium reverse movement, liquid glucose are fed to discharging certainly and move under hypersaturated state, because Cooling capacity is adequately utilized, and energy-saving effect is more significant, and primary crystallization rate is also increased to 65% by conventional 55%.

The first aspect of the utility model, provides:

A kind of technique of continuous crystallisation production glucose, includes the following steps:

Starch emulsion is prepared, then successively passes through liquefaction, saccharification, ion exchange desalination bleaching, evaporation and concentration, filtering, then pass through Crystallization is crossed, obtained material obtains glucose after being centrifuged, drying；

For crystallization process successively by the crystallization treatment of the multistage crystallizer being serially connected, syrup material is the knot from upper level Brilliant device enters the crystallizer of next stage；Chilled water is the crystallizer for entering upper level from the crystallizer of next stage；And each In the crystallizer of grade, syrup material is to flow from the top to the bottom, and chilled water is to flow from bottom to top.

In one embodiment, crystallization process is to use 4~10 grades of crystallizers being serially connected, more preferably 6~8 Grade.

In one embodiment, syrup material enters first order mould temperature and is preferably 44~48 DEG C.

In one embodiment, it is 7~12 DEG C that chilled water, which enters the temperature of afterbody crystallizer,.

In one embodiment, syrup material is when afterbody discharges 22~24 DEG C of temperature.

In one embodiment, temperature of the cooling water when the first order discharges is at 23~18 DEG C.

In one embodiment, the temperature that syrup material declines in every level-one crystallization process is no more than 5 DEG C, preferably not More than 3 DEG C；The heating of every level-one of cooling water is no more than 4 DEG C, preferably more than 2 DEG C.

In one embodiment, CO is added simultaneously from the top of the crystallizer of the first order₂, CO₂Additional amount volume with The volume of syrup material can be 1:100~150, CO₂The pressure of gas is controlled in 0.2~0.25MPa.

The second aspect of the utility model, provides:

A kind of continuous crystallisation produces the device of glucose, includes continuous crystalizer in device, comprising:

There are multiple crystallizers, crystallizer is connected between each other；It is equipped with syrup intlet at the top of crystallizer, in crystallizer Bottom is equipped with syrup outlet；

It is equipped with heat exchanger in the inside of crystallizer, the shell side of heat exchanger connects with chilled water import and chilled water outlet respectively It is logical；Chilled water import and chilled water outlet are located at the lower part and top of heat exchanger；

The syrup outlet of upper level crystallizer is connected to the syrup outlet of next stage crystallizer, the freezing of next stage crystallizer Water out is connected to the chilled water import of upper level crystallizer.

In one embodiment, product pump is also connected on syrup outlet, the crystallization obtained for conveying crystallizer Syrup.

In one embodiment, it is equipped with compressed gas import at the top of crystallizer, for blowing crystallizer inside It sweeps.

In terms of the third of the utility model, provide:

A kind of glucose production device, including above-mentioned continuous crystalizer, further includes:

With newborn tank, for preparing starch milk；

Liquefying reactor is connected to newborn tank, for carrying out liquefaction reaction to starch milk；

Be saccharified reactor, liquefying reactor is connected to, for carrying out saccharification reaction to liquefaction products；

Ion exchange resin column is connected to saccharification reactor, for carrying out ion exchange decoloration desalination to saccharification product；

Vapo(u)rization system is connected to the per-meate side of filter, is evaporated concentration for the permeate to filter；

Continuous crystalizer is connected to vapo(u)rization system, for carrying out crystallization treatment to syrup；

Centrifuge is connected to the discharge port of continuous crystalizer, for being centrifuged to crystallized stock, obtains glucose；

Double Air Dried Systems, for the glucose that centrifuge obtains to be dried.

In one embodiment, be connected on newborn tank and/or liquefying reactor amylase be added tank.

In one embodiment, carbohydrase being connected on saccharification reactor, tank is added.

In one embodiment, CO is additionally provided at the top of the crystallizer of the first order₂Mouth is added.

4th aspect of the utility model, provides:

Above-mentioned continuous crystalizer is for the purposes in crystallizing to Glucose Liquid.

Beneficial effect

1. reverse continuous crystallisation refers to: cold medium and the solute for needing cooling precipitation are phases in the direction of motion of material Anti- --- full adverse current flows to, i.e., material constantly completes cold and hot exchange in the case where moving hypersaturated state from discharging is fed to；

2. eight grades of series connection: referring to that eight crystallizers are connected in series together, form the system and device operation operation an of entirety. It is the single machine intermittently operated completed in an equipment and the operation of single machine continuous crystallisation different from traditional handicraft；

3. in terms of yield: new process compares traditional handicraft there has also been very big breakthrough, and one way crystallization yield is increased to from 55% 65%, total recovery, which is crystallized, from 85% is increased to 92%, it is horizontal in industry-leading；

4. in terms of cold balancing: because of cold and hot exchange, solute constantly feeds during traveling and is continuously precipitated, is nucleated, is long Greatly, movement discharging.Due to the variation of solute, release heat is precipitated in material and cooling medium takes away heat and reaches balance, passes in and out object Material reaches even running；

5. yield aspects: this new process mode is completed in set of system device, continuous operation, and yield is very high.It solves The drawbacks of traditional handicraft periodic crystallisation cannot reach continuous production and single machine continuous crystallisation low yield；

6. the maximum feature of new process is: being suitable for ultra-large type glucose production device, there is small investment, occupied area Small, one way and total crystallization yield are high, production capacity is big, unit cost is relatively low, height intelligent automation.

The quality index of crystal sugar has: contents of monosaccharides >=99.5%, molten sugar light transmittance >=98%, conductivity≤10 μ s/cm.And After above-mentioned new process, quality is significantly improved, and purity improves 0.2%, and light transmittance improves 1%, and conductivity averagely reduces by 0.4%, one Secondary crystallization yield improves 15%, and crystallization total recovery improves 7%, and total recovery reaches 92%.Process units system all realizes intelligence, The sugared construction investment of ton reduces by 50%, and process units realizes large (producing 350000 tons per year), and ton product price improves 20%, is produced into This reduction by 30%.Occupied area is only the 1/5 of traditional handicraft, and crystalline glucide amount is improved, and the utilization rate of raw material is mentioned It rises.Since technical process becomes more succinct, the consumption of public work is substantially reduced.Accomplish not only to improve product quality, but also Energy conservation and environmental protection is accomplished.

Above-mentioned series connection new process for continuous crystallization, embodies the integrated innovation of process route and process control, improves industry Technical level is mainly used for the production of high-purity crystallized glucose, and by many years application practice, device runs smoothly, quality In traditional handicraft, solves the urgent need of current crystal sugar process units enlargement, serialization.

New process advanced feature is compared with both at home and abroad:

Project	Foreign Advanced Lerel	Domestic existing level	The art of this patent is horizontal
				List covering device production capacity (ten thousand tons/year)	3~60,000 tons/year	60000 tons/year	350000 tons/year
Primary crystallization yield (%)	52~55%	55%	65%
				It crystallizes total recovery (%)	75%	85%	92%
The sugared investment of ton	It is high	It is low	It is ultralow
				Consumption of raw materials	It is high	In	It is low
Energy consumption	It is high	It is low	It is ultralow
				Waste heat recycling	80%	85%	100%
Occupied area	It is larger	Greatly	It is extra small

Detailed description of the invention

Fig. 1 is the device figure of the glucose crystallization of the offer of the utility model.

Fig. 2 is single-stage crystallization apparatus.

Fig. 3 is glucose production flow chart provided by the utility model.

Fig. 4 is glucose production plant system drawing provided by the utility model.

Fig. 5 is the particle size distribution figure of crystal sugar obtained in embodiment 1.

Fig. 6 is the HPLC map of crystal sugar obtained in embodiment 1.

Wherein, 1, with newborn tank；2, liquefying reactor；3, be saccharified reactor；4, ion exchange resin column；5, filter；6, Continuous crystalizer；7, centrifuge；8, double Air Dried Systems；9, vapo(u)rization system；61, crystallizer；62, compressed gas import；63, sugared Slurry inlet；64, syrup outlet；65, chilled water import；66, chilled water outlet；67, heat exchanger；68, product pump；69, water is cooling Device.

Specific embodiment

The utility model is described in further detail below by specific embodiment.But those skilled in the art will Understand, the following example is merely to illustrate the utility model, and should not be regarded as limiting the scope of the utility model.In embodiment not Indicate particular technique or condition person, according to the literature in the art described technology or conditions or according to product description into Row.Reagents or instruments used without specified manufacturer, being can be with conventional products that are commercially available.

Approximate language used herein can be used for modifying in entire disclosure and claims any quantity statement, can Permit being changed under conditions of not causing its relevant basic function to change.Therefore, it is repaired by term such as " about " The value of decorations is not limited to specified exact value.In at least some cases, approximate language can be with the instrument for measuring the value Precision it is corresponding.Unless indicating otherwise in context or sentence, otherwise range limit can be combined and/or exchange, and And this range is confirmed as and including all subranges contained herein.In addition in the operation embodiment or elsewhere In indicate except, the number of the amount of all expression compositions, reaction condition etc. used in specification and claims or Expression shall be construed as the modification by word " about " in all cases.

The value expressed using range format should be interpreted as not only including clearly enumerating as range in a flexible way The numerical value of limit value, but also including covering all single numbers or subinterval in the range, like each numerical value and sub-district Between be expressly recited out.For example, the concentration range of " about 0.1% to about 5% " should be understood as not only including clearly enumerating 4%) and subinterval (example the concentration of about 0.1% to about 5% further includes the single concentration in how (e.g., 1%, 2%, 3% and Such as, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%).

Word "include", "comprise" used herein, " having " or its any other variant are intended to cover non-exclusionism Including.E.g., including technique, method, article or the equipment for listing element are not necessarily limited by those elements, but may include it He is not explicitly listed or belongs to this technique, method, article or the intrinsic element of equipment.

The glucose that crystallization treatment is carried out required for the utility model refers to the grape obtained from amylorrhexis process Liquid glucose, reaction principle are to produce glucose using full enzyme method technique using cornstarch as raw material.Main technical process is as schemed Shown in 3.

Wherein, be to add water or starch milk to be transferred to 30~33% concentration in starch with newborn process, acid adding or alkali adjust pH value to 5.4~5.8, add alpha-amylase.

Liquefaction process mainly injection liquefaction twice, it is 105~108 DEG C of first time injection temperation, with pressure to hold time 15 points Clock, second 135~140 DEG C of injection temperation, it is with pressure to hold time 2~3 minutes, after flash distillation be added dropwise alpha-amylase total amount The 45% of 350ml/t butt, entering back into laminar flow tank (being kept for >=98 DEG C), the reaction was continued, total time >=120 minute of liquefying.Liquefaction is eventually Point DE value 13~17% sprays liquefied steam pressure requirement >=7.0kg/cm², injector requirement of liquefying for the first time is high pressure spray Emitter, secondary liquefaction injector are a heater, and flash distillation backpressure requirements are >=2.5kg/cm²。

Saccharifying needs will be cooled to 60~62 DEG C, adds diluted acid to adjust liquefier pH value 4.1~4.3, adds compounded saccharifying Enzyme 1000ml/t butt.Static reaction 48 hours, be saccharified terminal DE value >=98%, and compressed air stirring can be selected in saccharifying tank.Liquefaction Liquid, which cools down, can be selected shell and tube or plate heat exchanger.

Decolorization uses active carbon decoloring, and new active carbon is added in liquid glucose, and dosage is the 3% of butt.It is stirred in bleacher It mixes and enters filter press after twenty minutes.Active carbon chooses wet charcoal preferably, and filter press selects chip mechanical filter press or closed delivery sheet frame The environment of filter press, workshop easy to produce keeps cleaning.Liquid glucose after decoloration is limpid, transparent, colourless, non-foam and without carbon granule. Light transmittance >=96%.

Ion exchange resin treatment can be with desalination and decoloration, process flow are as follows: cation bed~anion bed~cation bed~anion bed.Flow For 2.5 BV/h, temperature≤55 DEG C, the conductivity of liquid glucose answers≤700 us/cm before handling.Pressure when operation in first column Answer≤2.0 ㎏/cm2.High 2.1~the 2.3m of resin layer.Card, device water cap and the quartz for being laid with certain altitude are arranged at ion-exchange column lower part Sand.Ion-exchange column will set middle comb, reduce the consumption of regenerative agent.After resin penetrates, the liquid glucose in column should be by clean compressed air pressure Tank or tune powder tank before best friend.The backwash of necessary big yield (5.0~8.0 BV/h) before regeneration, until the light transmittance of upper comb water outlet ≥96%.The dilute acid concentration of regenerative agent is 4~5%, diluted alkaline concentration 3~4%.Regeneration completes to want first slow (1.0~1.5 BV/ when elution H) afterwards fast (5.0~8.0 BV/h).The conductivity of after ion-exchange liquid glucose answers≤50 us/cm, pH value 3.8~4.5, and light transmittance >= 98%。

Evaporation process be by multiple-effect falling film evaporator by liquid glucose be concentrated to solid content be 72.5~73.5%.Heater work Work will keep continuity, the total pressure of steam >=0. 5Pma.One 80~90 DEG C of temperature of effect vaporization chamber sugar, two effect vaporization chamber sugar temperature 65~75 DEG C, 45~55 DEG C of triple effect evaporation room sugar temperature, all vapor condensed waters should all collect, and be mainly used for boiler and ion-exchange work Sequence (for eluting water temperature≤50 DEG C when resin).

Evaporating sugar-molasses syrup is filtered decoloration by the chip mechanical press through having applied paving layer of charcoal.The additive amount of active carbon (wet) For 0.5%/t butt.Filter cloth ensures that syrup does not leak carbon granule when being laid with.One underflow decoloration filters pressing function uses 30 hours, unloads The useless reusable Yu Qiandao bleaching process of charcoal.

After pervaporation and filtration treatment, liquid glucose carries out crystallization treatment.The utility model improves crystallization technique. Using continuous crystallization apparatus, continous way here refers to that multiple crystallizers are connected, and syrup material is by upper level After crystallizer carries out crystallisation by cooling processing, next stage is entered back into；And the chilled water employed in continous way crystallizer be by The upward first mobile of next stage；And syrup material is by top feed bottom discharge, chilled water on the crystallizer of every level-one It is to feed top discharge from bottom.Here multistage operations is preferably using using 6~8 grades of crystallizations.Syrup material enters the first order Mould temperature is preferably 44~48 DEG C, and the temperature that chilled water enters afterbody crystallizer is 7~12 DEG C；Syrup material is every The temperature declined during first degree crystalline controls the syrup in afterbody discharging no more than 5 DEG C, preferably more than 3 DEG C The temperature of material is controlled at 22~24 DEG C；The heating of every level-one of cooling water is controlled no more than 4 DEG C, preferably more than 2 DEG C Go out the temperature of cooling water at 23~18 DEG C in the first order.

Above-mentioned operating process, syrup material are that on the one hand crystal grain can be made in the process of crystallization by flowing downward using In, with naturally fall during grow, the partial size of the particle of obtained crystal grain is bigger, on the other hand, since chilled water is It is fed from the bottom of crystallizer, the temperature of bottom is lower, glucose can be made to have the more sufficient time to be crystallized, obtained knot Brilliant yield is significantly improved.

In one embodiment, during crystallization, CO is added simultaneously from the top of the crystallizer of the first order₂, with sugar Slurry material moves downward simultaneously, can adjust the Growing Process of Crystal Particles in crystallization process, and average grain diameter, the knot of particle can be improved Brilliant yield and the distribution variation coefficient for reducing partial size.CO₂The volume of additional amount and the volume of syrup material can be 1:100 ~150, CO₂The pressure of gas is controlled in 0.2~0.25MPa.

Its operating process is as depicted in figs. 1 and 2.

Material: liquid glucose slurry continuously enters first order crystallizer by top, and sugar entering temperature is 46 DEG C.Inside tank with The freezing complete heat of water coke slurry is got by tank bottom, then is entered by the tank deck of second level crystallizer, and tank bottom is got.It is concatenated with this in this way Mode sequentially enters next stage crystallizer, until the 8th grade of crystallizer gets glucose massecuite.

Chilled water: 7~12 DEG C of chilled water is inversely continuously entered the inner disk of the 8th grade of crystallizer by the 8th group of heat exchanger Pipe, by bottom plate water inlet tube, the material that top coil pipe is discharged and the 8th grade of crystallizer enters from top to down carries out reverse heat-exchange. Water outlet returns to the 8th group of heat exchanger, enters the 7th group after entering the chilled water heat exchange of the 8th group of heat exchanger, then with water intake mode Heat exchanger is exchanged heat in a manner of bottom in and top out with the material of upper entering and lower leaving by the 7th grade of crystallizer coil pipe.And so on, together Sample sequentially enters next stage heat exchanger in series, until first group of heat exchanger water outlet returns to chilled water return main's line.

Reaction is whole, and material enters from the first order, from top to bottom moves in tank；Chilled water enters from the 8th grade, through changing Hot device from bottom to top moves in tank inner coil pipe, and material and chilled water whole process are without directly contacting.Material, which is precipitated, releases heat, freezing Water absorbs heat.I.e. the most hot material of the first order and the 8th grade of temperature become highest chilled water heat exchange, after the 8th grade of heat exchange most The cool the coldest chilled water of material and the first order exchanges heat, and every first degree crystalline heat exchange, the temperature difference is all controlled in t=3 DEG C △, energy Keep weighing apparatus, whole device even running, continuous crystallisation.

Macroscopically: the material of whole device continuously moves from front to back, and crystallization is precipitated；Chilled water is inversely transported from back to front It is dynamic, it exchanges heat with material.Microcosmic upper: in the crystallizer of every level-one, material is from top to bottom continuously moved；Chilled water is in coil pipe In continuously exchange heat therewith from the bottom to top；In heat exchanger, chilled water water outlet can carry out Continuous Heat Transfer with water inlet again, and energy obtains It recycles.No matter from macroscopically or it is microcosmic on, in the state that material and chilled water are all in continuous and movement, be not only able to Volume increase, and the microbiological contamination for avoiding material is rotten.The utility line of auxiliary plays the role of escorting, and steam can Whole process sterilize without dead angle；Aseptic compressed air is purged and is completely cut off outside air pollution；Recirculated water can be in cold day It exchanges heat instead of chilled water；Whole process has been laid with material and chilled water and public work main pipe line, (as overhauled under specific condition A certain crystallizer), device still can run without interruption.

In the degree of automation: disengaging material pipeline and chilled water pipeline on all be provided with regulating valve and switch valve, and with phase The liquidometer and thermometer of pass have carried out chain, can automatically control disengaging inventory and chilled-water flow, save manpower behaviour Make, the operation of whole device is made to become more accurate and steady.

Based on above operating process, shown in the structure chart 1 of used continuous crystalizer 6, comprising:

There are multiple crystallizers 61, crystallizer 61 is connected between each other；It is equipped with syrup intlet 63 at the top of crystallizer 61, The bottom of crystallizer 61 is equipped with syrup outlet 64；

The inside of crystallizer 61 be equipped with heat exchanger 67, the shell side of heat exchanger 67 respectively with chilled water import 65 and chilled water 67 connection of outlet；Chilled water import 65 and chilled water outlet 67 are located at the lower part and top of heat exchanger 67；

The syrup outlet of upper level crystallizer is connected to the syrup outlet of next stage crystallizer, the freezing of next stage crystallizer Water out is connected to the chilled water import of upper level crystallizer.

In one embodiment, it is also connected with product pump 68 on syrup outlet 64, is obtained for conveying crystallizer 61 Crystallization syrup.

In one embodiment, further include water cooler 69, be connected to chilled water import 65 and chilled water outlet 67, use It is cooled down in chilled water.

In one embodiment, it is equipped with compressed gas import 62 at the top of crystallizer 61, inside to crystallizer 61 It is purged.

The utility model provide include above-mentioned continuous crystalizer 6 glucose production device, as shown in Figure 3, comprising:

With newborn tank 1, for preparing starch milk；

Liquefying reactor 2 is connected to newborn tank 1, for carrying out liquefaction reaction to starch milk；

Be saccharified reactor 3, liquefying reactor 2 is connected to, for carrying out saccharification reaction to liquefaction products；

Ion exchange resin column 4 is connected to saccharification reactor 3, for carrying out ion exchange decoloration desalination to saccharification product；

Vapo(u)rization system 9 is connected to the per-meate side of filter 5, is evaporated at concentration for the permeate to filter 5 Reason；

Continuous crystalizer 6 is connected to vapo(u)rization system 9, for carrying out crystallization treatment to syrup；

Centrifuge 7 is connected to the discharge port of continuous crystalizer 6, for being centrifuged to crystallized stock, obtains glucose；

Double Air Dried Systems 8, the glucose for obtaining to centrifuge 7 are dried.

In one embodiment, be connected on newborn tank 1 and/or liquefying reactor 2 amylase be added tank.

In one embodiment, carbohydrase being connected on saccharification reactor 3, tank is added.

In one embodiment, the top of the crystallizer 61 of the first order is additionally provided with CO₂Mouth is added.

It is that amylase solution obtains that Glucose Liquid used by state Behavior of Continuous Crystallization Processes is carried out in following embodiment, saccharified liquid DX value 95.5%, saccharified liquid concentration 71%ds,

Embodiment 1

Using 8 grades of series connection continuous crystalizers, liquid glucose is warming up to 46 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, the temperature of chilled water is It 8~9 DEG C, is added from the 8th grade of crystallizer, the lower part of the coil condenser in each crystallizer is chilled water import, top Chilled water outlet out, chilled water flow from bottom to top, and the crystallizer of upper level is flowed to from the crystallizer of next stage；Pass through Flow is adjusted, after even running, the heating of every level-one of cooling water is no more than 2 DEG C, and syrup material is in every level-one crystallization process The temperature of decline is no more than 3 DEG C, 23 DEG C of chilled water outlet temperature at the first order, and the 8th grade 24 DEG C of syrup outlet temperature.

Embodiment 2

Using 8 grades of series connection continuous crystalizers, liquid glucose is warming up to 44 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, the temperature of chilled water is It 7~8 DEG C, is added from the 8th grade of crystallizer, the lower part of the coil condenser in each crystallizer is chilled water import, top Chilled water outlet out, chilled water flow from bottom to top, and the crystallizer of upper level is flowed to from the crystallizer of next stage；Pass through Flow is adjusted, after even running, the heating of every level-one of cooling water is no more than 2 DEG C, and syrup material is in every level-one crystallization process The temperature of decline is no more than 3 DEG C, 24 DEG C of chilled water outlet temperature at the first order, and the 8th grade 22 DEG C of syrup outlet temperature.

Embodiment 3

Using 6 grades of series connection continuous crystalizers, liquid glucose is warming up to 44 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, the temperature of chilled water is It 7~8 DEG C, is added from the 6th grade of crystallizer, the lower part of the coil condenser in each crystallizer is chilled water import, top Chilled water outlet out, chilled water flow from bottom to top, and the crystallizer of upper level is flowed to from the crystallizer of next stage；Pass through Flow is adjusted, after even running, the heating of every level-one of cooling water is no more than 3 DEG C, and syrup material is in every level-one crystallization process The temperature of decline is no more than 4 DEG C, 23 DEG C of chilled water outlet temperature at the first order, and the 8th grade 23 DEG C of syrup outlet temperature.

Embodiment 4

Using 6 grades of series connection continuous crystalizers, liquid glucose is warming up to 46 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, the temperature of chilled water is It 9~10 DEG C, being added from the 6th grade of crystallizer, the lower part of the coil condenser in each crystallizer is chilled water import, on Portion goes out chilled water outlet, and chilled water flows from bottom to top, and the crystallizer of upper level is flowed to from the crystallizer of next stage；It is logical Toning amount of restriction, after even running, the heating of every level-one of cooling water is no more than 3 DEG C, and syrup material is in every level-one crystallization process The temperature of middle decline is no more than 4 DEG C, 23 DEG C of chilled water outlet temperature at the first order, and the 8th grade 23 DEG C of syrup outlet temperature.

Embodiment 5

Using 8 grades of series connection continuous crystalizers, liquid glucose is warming up to 46 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, while in first order knot The top of brilliant device is pressed into CO₂Compressed gas, air pressure 0.2MPa, it is that syrup is added the 1/120 of volume that volume, which is added, the temperature of chilled water It is 8~9 DEG C, is added from the 8th grade of crystallizer, the lower part of the coil condenser in each crystallizer is chilled water import, on Portion goes out chilled water outlet, and chilled water flows from bottom to top, and the crystallizer of upper level is flowed to from the crystallizer of next stage；It is logical Toning amount of restriction, after even running, the heating of every level-one of cooling water is no more than 2 DEG C, and syrup material is in every level-one crystallization process The temperature of middle decline is no more than 3 DEG C, 23 DEG C of chilled water outlet temperature at the first order, and the 8th grade 24 DEG C of syrup outlet temperature.

Embodiment 6

Using 8 grades of series connection continuous crystalizers, liquid glucose is warming up to 44 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, while in first order knot The top of brilliant device is pressed into CO₂Compressed gas, air pressure 0.2MPa, it is that syrup is added the 1/120 of volume that volume, which is added, the temperature of chilled water It is 7~8 DEG C, is added from the 8th grade of crystallizer, the lower part of the coil condenser in each crystallizer is chilled water import, on Portion goes out chilled water outlet, and chilled water flows from bottom to top, and the crystallizer of upper level is flowed to from the crystallizer of next stage；It is logical Toning amount of restriction, after even running, the heating of every level-one of cooling water is no more than 2 DEG C, and syrup material is in every level-one crystallization process The temperature of middle decline is no more than 3 DEG C, 24 DEG C of chilled water outlet temperature at the first order, and the 8th grade 22 DEG C of syrup outlet temperature.

Reference examples 1

Difference with embodiment 1 is: chilled water is added from the lower part of first order crystallizer, and enters second level crystallizer Lower part, until being flowed out from the top of afterbody.

Using 8 grades of series connection continuous crystalizers, liquid glucose is warming up to 46 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, the temperature of chilled water is 8~9 DEG C, condenser is flowed into from the bottom of first order crystallizer, and flow out from upper end, enter back into the condenser of second level crystallizer Bottom, successively flowed out from the top of the 8th grade of crystallizer condenser, i.e., chilled water flows between grade and grade with syrup identical, And it is flowed between single-stage opposite；By adjusting flow, after even running, the heating of every level-one of cooling water is no more than 2 DEG C, sugar The temperature that slurry material declines in every level-one crystallization process is no more than 3 DEG C, 23 DEG C of chilled water outlet temperature at the first order, and the 8th grade 24 DEG C of syrup outlet temperature.

Reference examples 2

Difference with embodiment 1 is: chilled water is added from the top of first order crystallizer, and enters second level crystallizer Top, until being flowed out from the lower part of afterbody.

Using 8 grades of series connection continuous crystalizers, liquid glucose is warming up to 46 DEG C, and add a small amount of crystal seed, with 50 ton/hours of speed Degree is added from the top of first order crystallizer, flows downward, and successively flow from downward first degree crystalline device, the temperature of chilled water is 8~9 DEG C, condenser is flowed into from the top of first order crystallizer, and flow out from lower end, enter back into the condenser of second level crystallizer Top, successively flowed out from the lower part of the 8th grade of crystallizer condenser, i.e., chilled water flows between grade and grade with syrup identical, And it is flowed between single-stage also identical；By adjusting flow, after even running, the heating of every level-one of cooling water is no more than 2 DEG C, The temperature that syrup material declines in every level-one crystallization process is no more than 3 DEG C, 23 DEG C of chilled water outlet temperature at the first order, and the 8th 24 DEG C of temperature of syrup outlet of grade.

Reference examples 3

Difference with embodiment 1 is: being operated using single machine continuous crystallisation.

Using the vertical crystallizer of separate unit, liquid glucose is warming up to 46 DEG C, and add a small amount of crystal seed, is added with the speed of 200L/min Enter at the top of crystallizer, 18~19 DEG C of chilled water is added from the bottom of vertical crystallizer, and adjusting flow velocity flows chilled water from top 30~32 DEG C of temperature when out, syrup are flowed out from bottom with 24 DEG C of temperature.

Glucose crystallization material obtained in the above various embodiments and reference examples is centrifuged using centrifuge, and is carried out It is dry, obtain glucose.Centrifugal process wash 3 times, washing temperature is 30 DEG C, be centrifuged to wet sugar moisture in 14wt% hereinafter, from Wet sugar after heart separation is sent at gas flow dryer charging, and mixes wind-warm syndrome after 85~90 DEG C of (wind-warm syndrome) hot airs Reach 60~70 DEG C, through primary drying, obtains satisfactory commerieal sugar after primary cooling.

The partial size of glucose

Glucose crystal sample is constituted according to certain partial size allocation proportion.Sample stays in after one group of sieve screens Particle cumulative percent on sieve can draw straight line, the i.e. grain of sample to the relationship of partial size on normal probability paper Diameter Normal Distribution, the normal probability density function of particle diameter distribution are as follows:

Wherein, x is the random sample value of this distribution extraction, i.e. size of microcrystal；μ is the abscissa of curve highest point, referred to as The mean value of normal distribution, curve are symmetrical to μ；σ is the standard deviation of normal distribution.

The coefficient of variation Cv of crystal is a parameter for describing crystal particle diameter distribution, and calculation formula is

In formula, the 1/2 of the difference of corresponding abscissa that δ is probability P when being respectively 16%t 84% is, it is specified that P is 16%, 50%, 84% Corresponding interval endpoint is respectively x16, x50 and x84, obtains Cv such as following formula and calculates:

The average grain diameter of glucose crystal grain obtained in the above various embodiments and reference examples uses 2000 type of Mastersize Laser particle analyzer is detected, and average grain diameter and the coefficient of variation are as shown in the table, and the glucose being prepared in embodiment 1 is brilliant The particle size distribution figure of grain is as shown in Figure 4.

It can be seen that the multistage continuous crystallisation for using the utility model obtained by embodiment 1 and comparing for reference examples 3 Glucose crystal grain obviously has bigger average grain diameter relative to traditional vertical single stage crystallization, by embodiment 1,2 and implements The comparison of example 3,4 is as can be seen that the partial size for crystallizing obtained crystal grain using 8 grades is significantly greater than 6 grades of crystallizations, it may be possible to due to passing through The growth of crystal grain can be effectively facilitated by adjusting cooling rate and crystallization time；It can be seen by embodiment 1 and the comparison of reference examples 1 Out, the reverse flow mode by the syrup and chilled water in the utility model between at different levels, can effectively improve crystallization The partial size of effect, the glucose made is bigger, can be seen that the crystallization in single-stage by the comparison of reference examples 1 and reference examples 2 In device, the reverse flow of chilled water and syrup can effectively improve crystallization effect, improve the partial size of crystal grain and reduce distribution The coefficient of variation, make to be distributed narrower；By the comparison of embodiment 1,2 and embodiment 5,6 as can be seen that by using in crystallization It is passed through CO in the process₂The growing environment that can change grain surface, the grain growth made is more preferable, have bigger partial size with And narrower distribution.

The purity of glucose

It is characterized using content of the HPLC method to crystal glucose, using Waters 1525HPLC instrument, TU1900 is bis- Light beam ultraviolet photometer, chromatographic column Ultimate XB-C18 column, 4.5mm × 250mm × 2.5 μm, mobile phase acetonitrile-water (65: 35)；Flow velocity 1ml/min；30 DEG C of column temperature；Detection wavelength 209nm；10 μ l are measured into school, number of theoretical plate is not less than 4500, embodiment 1 Obtained in crystal sugar HPLC map it is as shown in Figure 6.In addition, taking 10g glucose to be dissolved in 100g distilled water, using light splitting Photometric determination light transmittance measures the conductivity of molten sugar using conductivity meter.

It can see by the comparison of embodiment 1,2 and embodiment 3,4, the process crystallized using 8 grades is due to grain growth Process is more uniform, and the impurity that can be effectively prevented in syrup resides in crystal sugar, and the quality of the crystal sugar made is more It is good.It can be seen that the quality of the crystal sugar obtained using multistage continuous adverse current crystallisation by cooling by embodiment 1,2 and reference examples It is also significantly better than the crystal sugar that chilled water is crystallized with syrup co-flow.

Percent crystallization in massecuite

Using glucose content calculating crystallization rate in crystallization sugar weight/crystallization syrup.

As can be seen from the above table, the percent crystallization in massecuite for the glucose that the crystallization of the continuous adverse current type of the utility model obtains can be with Reach 92% or more, better than the reverse-flow continuous crystallisation of co-flow and part in reference examples 1-3, also superior to reference examples 3 85% percent crystallization in massecuite of vertical crystallizing tower in the prior art.

Claims (7)

1. a kind of continuous crystalizer for producing glucose, which is characterized in that the continuous crystalizer (6) includes:

Have multiple crystallizers (61), crystallizer (61) is connected between each other；Syrup intlet is equipped at the top of crystallizer (61) (63), syrup outlet (64) are equipped in the bottom of crystallizer (61)；

Be equipped with heat exchanger (67) in the inside of crystallizer (61), the shell side of heat exchanger (67) respectively with chilled water import (65) and cold Freezing water outlet (66) connection；Chilled water import (65) and chilled water outlet (66) are located at the lower part of heat exchanger (67) and upper Portion；

The syrup outlet of upper level crystallizer is connected to the syrup outlet of next stage crystallizer, and the chilled water of next stage crystallizer goes out Mouth is connected to the chilled water import of upper level crystallizer.

2. the continuous crystalizer of production glucose according to claim 1, which is characterized in that on syrup outlet (64) also Product pump (68) are connected with, the crystallization syrup obtained for conveying crystallizer (61).

3. the continuous crystalizer of production glucose according to claim 1, which is characterized in that at the top of crystallizer (61) Equipped with compressed gas import (62), for being purged to crystallizer (61) is internal.

4. a kind of glucose production device, including continuous crystalizer described in claim 1 (6), which is characterized in that further include:

With newborn tank (1), for preparing starch milk；

Liquefying reactor (2) is connected to newborn tank (1), for carrying out liquefaction reaction to starch milk；

It is saccharified reactor (3), liquefying reactor (2) is connected to, for carrying out saccharification reaction to liquefaction products；

Ion exchange resin column (4) is connected to saccharification reactor (3), for carrying out ion exchange decoloration desalination to saccharification product；

Filter (5), is connected to the discharge port of exchange resin column (4), for being filtered to the liquid glucose after ion-exchange treatment Removal of impurities processing；

Vapo(u)rization system (9), is connected to the per-meate side of filter (5), for being evaporated at concentration to the permeate of filter (5) Reason；

Continuous crystalizer (6) is connected to vapo(u)rization system (9), for carrying out crystallization treatment to syrup；

Centrifuge (7), is connected to the discharge port of continuous crystalizer (6), for being centrifuged to crystallized stock, obtains glucose；

Double Air Dried Systems (8), the glucose for obtaining to centrifuge (7) are dried.

5. glucose production device according to claim 4, which is characterized in that with newborn tank (1) and/or liquefying reactor (2) it is connected with amylase on, tank is added.

6. glucose production device according to claim 4, which is characterized in that be connected with saccharification in saccharification reactor (3) Tank is added in enzyme.

7. glucose production device according to claim 4, which is characterized in that the top of the crystallizer (61) of the first order is also Equipped with CO₂Mouth is added.